Sulfuric Acid → 3-Methyl-1-decanol

HRID 444334ノート

反応式

HRID 444334 の反応式
C([O:3][C:4](=O)[CH2:5][CH:6]([CH3:14])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])C.[H-].[Al+3].[Li+].[H-].[H-].[H-].S(=O)(=O)(O)O>CCOCC>[CH3:14][CH:6]([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])[CH2:5][CH2:4][OH:3]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 560492Ethyl 3-methyldecanoateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 150549973-Methyl-1-decanol収率 88.9%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

740 g (3.46 mols) 3-methyl-decanoic acid ethyl ester, dissolved in 600 ml ether, are added while cooling to a suspension of 72 g (1.89 mols) lithium aluminium hydride in 600 ml ether. After the addition has ended the reaction mixture is heated for one hour to reflux temperature, is then hydrolysed and acidified with sulphuric acid. The organic phase is separated off, the aqueous phase is extracted with ether and the combined organic phases are freed from solvent. The destillation of the residue gives 529.5 g 3-methyldecanol (b.p.0.3 :83° C.), corresponding to a yield of 88.9% of theory.

後処理

  1. additionare added
  2. additionAfter the addition
  3. temperatureis heated for one hour
  4. temperatureto reflux temperature
  5. customThe organic phase is separated off
  6. extractionthe aqueous phase is extracted with ether

出典と根拠

ORDレコード
ord-a609af37aa584653b6c9039ec5b44396
出典データセット
uspto-grants-1981_04
特許番号
US04263459

反応ノート

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